I am analysing Triethylamine content in drug substances. I wellcome comments about the methodology developed recently by me.
Column: DB-1(30mX0.53mmX1.5µ).
Sample: 1 g dissolved with 1 mL of 4N NaOH solution diluted with 1 mL water. 2 mL of Internal Standard solution (in ethylacetatesolvent ).
shaked gently for one minute. organic layer separated and injected (1 µl, splitless at 125°C) into a gas chromatograph using the following oven programme, 40°C//5mts -- 8°C/min. -- 100°C. Detector : FID (250°C)
Standard : 1 mL of Std (0.2mg/mL) + 1 mL of water. 2 mL of Internal standard solution.
i am half-way through of the validation of this method and hence i call for the discussions.
vijayaragavan
orchid chemicals and pharmaceuticals limited
Reseach and Development centre,
chennai, India

Hi, Vijay!
I'm analysing triethylamine too. By the same method I'm doing n,n-dimethylaniline.
My method:
Column: Ultra-2 25m 0.32mm 0.5micrometer
Sample: 0.2 g dissolve in 2 ml of water, add 0.2 ml of 10N NaOH and n-hexane. Shake one minute. Inject hexane phase.
Standard: 2 ml(0.002% of triethylamine and 0.002% n,n-dimethylaniline in water) + n-hexane + 0.2 ml 10N NaOH
Injection volume is 1 microliter, splitless. Head pressure 40 kPa. 40 d during 5 minutes, then rise temp. to 250 d.
I get good linearity for n,n-dimethylaniline and worse for triethylamine. RSD is less than 5%.
I think ethylacetate will be hydrolysed. You did not mention what you are using as the internal standard.

Vijay:

BANDCHUD!!!!!


Have a nice day!